CN101502789A - Method for preparing magnetic active carbon composite material for water processing - Google Patents
Method for preparing magnetic active carbon composite material for water processing Download PDFInfo
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- CN101502789A CN101502789A CNA2009100459562A CN200910045956A CN101502789A CN 101502789 A CN101502789 A CN 101502789A CN A2009100459562 A CNA2009100459562 A CN A2009100459562A CN 200910045956 A CN200910045956 A CN 200910045956A CN 101502789 A CN101502789 A CN 101502789A
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Abstract
The invention provides a method for preparing a magnetic active carbon composite material for water treatment in the technical field of environmental purification. The method comprises the following steps: mixing active carbon and corresponding metal salt solution, and generating magnetic nano granules in pore canals of the active carbon in situ by using the characteristics of instantaneous high temperature, high pressure, high cooling speed and the like generated by ultrasonic waves; and filtering and drying the obtained compound, and treating the compound at high temperature to form the magnetic active carbon composite material, wherein the magnetic material accounts for 15 to 50 percent in the whole material in terms of weight percentage, and the active carbon material accounts for 85 to 50 percent. The invention provides a new method for generating magnetic nano particles in the pore canals of the active carbon; and the prepared magnetic active carbon keeps larger specific surface area, reserves the open pore canals from the active carbon, removes organic substances and inorganic heavy metal ions in water treatment, and is easy for magnetic separation and convenient to recover.
Description
Technical field
That the present invention relates to is the preparation method of a kind of composite material and preparation method thereof of depollution of environment technical field, particularly a kind of magnetic active carbon composite material for water processing.
Background technology
Absorbent charcoal material is meant that a class has the porous material of highly developed specific area and porosity.The raw material of active carbon can be agricultural wastes, as wooden unit, coconut husk, rice husk, wild rice stem leaf, also can be synthetic materials, as synthetic rubber, foamed plastics etc.These materials decompose and remove non-carbonizable substance by high temperature cabonization, retain constitutionally stable charcoal body, and this charcoal body has preliminary pore structure, and the activation process through physics or chemistry just obtains the pore structure prosperity again, and specific area is up to 1000-3000m
2.g
-1Absorbent charcoal material.Therefore, active carbon all has very strong adsorption capacity to inorganic or organic substance and the colloidal solid etc. in gas, the solution, has good adsorption performance and stable chemical property, can anti-strong acid, highly basic, stand water logging, high temperature, high pressure effect, and be difficult for broken.Utilize its physical absorption, chemisorbed, biological absorption, catalysis, performances such as oxidation and reduction can be removed multiple polluter such as organic impurity in the waste water, metal ion etc.Active carbon is used in water treatment and is mainly reflected in aspect three.The first, the purification of source of sewage is with organic matter, color, stink, oil, phenol etc. in the charcoal absorption water; Second, organic industrial sewage is handled, because active carbon has outstanding removal ability to the organic matter in the water, some are difficult to by biodegradable organic matter unique removal effect be arranged more and be used in leather-making waste water processing, the wastewater treatment of papermaking dye chemical industry, Treatment of Coking Effluent and other treatment of Organic Wastewater.The 3rd, inorganic Industrial Wastewater Treatment, active carbon has the selection adsorption capacity for inorganic heavy metal ion in the waste water.In addition, it all has extremely extensive and important purposes at aspects such as food processing, pharmacy, chemistry, metallurgy, agriculturals.
But, because the fineness ratio of active carbon is less, in application, be difficult to separation, recycling, become a difficult problem of practical application.In order to address this problem, the someone utilizes ferrous salt and active carbon blend, and the method for sintering prepares Fe
3O
4-active carbon compound is given active carbon reaches separation with magnetic effect.Regrettably in preparation process, used ferrous salt instability, oxidized easily, cause severe reaction conditions.Simultaneously, owing to be solution blended process, the Fe that makes
3O
4Particle is grown in the outer surface of active carbon, oxidation by air easily, magnetic instability.The more important thing is, be grown in the Fe of outer surface
3O
4Particle is reunited under the effect of external environment easily, and the duct of blocking portion active carbon descends the composite specific surface of gained greatly, thereby has limited the application of material aspect absorption.
Find through literature search prior art, Chinese invention patent publication number CN1500736A, this patent is mixed with MnFe with metal salt solution and active carbon
2O
4Or CuFe
2O
4Compound with active carbon.Though, use MnFe
2O
4Or CuFe
2O
4Replace Fe
3O
4Can solve the magnetic property stability problem, but the magnetic particle that the method for this solution and active carbon blend produces is grown in the outer surface of active carbon, can not make full use of the high-ratio surface of active carbon, the magnetic particle of outer surface is reunited easily simultaneously, is unfavorable for practical application.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of magnetic active carbon composite material for water processing is provided, in the duct of absorbent charcoal material, generate magnetic nano-particle, the preparation magnetic active carbon, make the composite for preparing have bigger specific area, have stronger absorption property, simultaneously, can realize the function of utilizing magnetic from solution, to separate.
The present invention is achieved through the following technical solutions, the present invention includes following steps:
The first step stirs the Powdered Activated Carbon material in nitric acid, wash with deionized water, and is dry then.
Second step took by weighing the first step and handles the back absorbent charcoal material, join in the metal salt solution, the mole dosage of slaine be active carbon amount of substance 0.24-2.88 doubly, at room temperature ultrasonic, obtain powder sample, wash with water, dry then.
The 3rd step, the second step gained material is put into high temperature furnace, be heated to 500-800 ℃ under the blanket of nitrogen, be incubated 1-5 hour, just obtain magnetic active carbon composite material at last, according to the consumption of slaine, the magnetic material of acquisition (refer to generate tri-iron tetroxide, nickel oxide, manganese oxide) is 15-50% at the percentage by weight of magnetic active carbon composite material, absorbent charcoal material 85-50%.
Can control the power of magnetic by the consumption of slaine, ultrasonic time.
Described absorbent charcoal material can be the absorbent charcoal material various apertures, different shape that plants such as husk, wild rice stem leaf, coconut husk, wood chip or synthetic materials such as rubber, foam are made.
Described stirring, its temperature are 70-90 ℃, mixing time 1-6 hour, are preferably 3-5 hour.
Described metal salt solution is metal salt solutions such as iron, nickel, manganese, and water soluble comprises: sulfate, hydrochloride, nitrate, permanganate etc.Being not limited to above-mentioned several material, comprising that all can generate the slaine of magnetic metal or metal oxide by ultrasonic method, can be the combination of one or more salt.
The mole dosage of described slaine be active carbon amount of substance 0.24-2.88 doubly.
Described at room temperature ultrasonic, 0.25-4 hour its time.
Described insulation, its time is 1-5 hour.
The present invention utilizes hyperacoustic special performance, the nano particle growth in situ that will have magnetic function in the duct of active carbon, thereby obtain having concurrently the magnetic active carbon composite material of Magnetic Isolation function and absorption property.This material has kept the open pore passage structure of active carbon, for the transmission of material provides passage, organic and inorganic pollutant is had the good adsorption performance.
Utilize the inventive method, can obtain having good magnetic response, utilize that magnetic separation method separates, the absorbent charcoal material of recycling.Compared with former technology, ultrasonic powerful effect is uniformly dispersed magnetic particle, makes the bigger specific surface of maintenance of the composite of gained.Because magnetic particle is grown in the inner surface of absorbent charcoal material, is not easy oxidation by air, make magnetic property stable.Simultaneously, the supporting role of active carbon body of wall makes the magnetic particle that is created on inner surface be difficult for reuniting,
Technology of the present invention is simple, magnetic active carbon adsorption treatment waste water, and not only adsorbance is bigger, and can also make quick pollution-free separation.Therefore, the material processed waste water of preparation has advantages such as applied range, good, the recyclable useful material of treatment effect, adsorbent be reusable.
The specific embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Ultrasonic synthetic 15% Fe that contains
3O
4Magnetic active carbon composite material.
The active carbon bubble was stirred 1 hour under 70 ℃ in the 63wt% red fuming nitric acid (RFNA), filter, washing.Take by weighing above active carbon 5g, be dissolved in 200ml, in the iron nitrate solution of 0.5M, stir.Under the room temperature ultrasonic 15 minutes, filter.Wash the powder of gained with water one to twice, oven dry.Be put in the high temperature furnace and be heated to 500 ℃ under the nitrogen atmosphere, be incubated 3 hours.Promptly obtain the tri-iron tetroxide absorbent charcoal composite material, wherein Fe
3O
4Content 15%, specific area 800m
2g
-1, behind the adsorbing phenol, carry out magnetic with magnet and separate.
Embodiment 2
Ultrasonic synthetic 30% Fe that contains
3O
4Magnetic active carbon composite material.
The active carbon bubble was stirred 3 hours under 80 ℃ in the 63wt% red fuming nitric acid (RFNA), filter, washing.Take by weighing above active carbon 5g, be dissolved in 200ml, in the iron nitrate solution of 3M, stir.Under the room temperature ultrasonic 1.5 hours, filter.Wash the powder of gained with water one to twice, oven dry.Be put in the high temperature furnace and be heated to 650 ℃ under the nitrogen atmosphere, be incubated 3 hours.Promptly obtain the tri-iron tetroxide absorbent charcoal composite material, wherein Fe
3O
4Content 30%, specific area 770m
2g
-1Under 25 ℃, 1g magnetic activated carbons composite can be removed the 321mg methylene blue at most.Absorbent charcoal material absorption property than identical specific area is far better.Can also use magnet to separate fast.
Embodiment 3
Ultrasonic synthetic 40% Fe that contains
3O
4Magnetic active carbon composite material.
The active carbon bubble was stirred 6 hours under 90 ℃ in 63% red fuming nitric acid (RFNA), filter, washing.Take by weighing above active carbon 5g, be dissolved in 200ml, in the iron nitrate solution of 4M, stir.Under the room temperature ultrasonic 4 hours, filter.Wash the powder of gained with water one to twice, oven dry.Be put in the high temperature furnace and be heated to 800 ℃ under the nitrogen atmosphere, be incubated 3 hours.Promptly obtain the tri-iron tetroxide absorbent charcoal composite material, wherein Fe
3O
4Content 50%, specific area 650m
2g
-1, after copper ion absorption, this composite can use magnet to separate from solution fast.
Embodiment 4
Ultrasonic synthetic 32% Fe that contains
3O
4Magnetic active carbon composite material.
The active carbon bubble was stirred 5 hours under 90 ℃ in 63% red fuming nitric acid (RFNA), filter, washing.Take by weighing above active carbon 5g, be dissolved in 200ml, in the monsel solution of 1M, stir.Under nitrogen protection, ultrasonic 4 hours of room temperature is filtered.Wash the powder of gained with water one to twice, oven dry.Be put in the high temperature furnace and be heated to 700 ℃ under the nitrogen atmosphere, be incubated 5 hours.Promptly obtain the tri-iron tetroxide absorbent charcoal composite material, wherein Fe
3O
4Content 32%, specific area 745m
2g
-1, this composite can use magnet to separate from solution fast.
Embodiment 5
The ultrasonic synthetic 25%NiO that contains
2Magnetic active carbon composite material.
The active carbon bubble was stirred 4 hours under 80 ℃ in the 63wt% red fuming nitric acid (RFNA), filter, washing.Take by weighing above active carbon 5g, be dissolved in 200ml, in the nickel chloride solution of 4M, stir.Under the room temperature ultrasonic 1 hour, filter.Wash the powder of gained with water one to twice, oven dry.Be put in the high temperature furnace and be heated to 700 ℃ under the nitrogen atmosphere, be incubated 3 hours.Promptly obtain the nickel oxide absorbent charcoal composite material, the content 25% of nickel oxide wherein, specific area 720m
2g
-1Difference is measured this composite join in the variable concentrations copper ion solution, behind the 24h that in shaking table, vibrates under 25 ℃, with the content of atomic absorption spectroscopy determination copper ion in the aqueous solution.Under the experiment condition, the optimal adsorption value of this composite is 28mg.g
-1Carrying out magnetic after the absorption separates.
Embodiment 6
Ultrasonic synthetic 45% NiO that contains
2Magnetic active carbon composite material.
The active carbon bubble was stirred 3 hours under 90 ℃ in the 63wt% red fuming nitric acid (RFNA), filter, washing.Take by weighing above active carbon 5g, be dissolved in 200ml, in the nickel chloride solution of 5M, stir.Under the room temperature ultrasonic 2 hours, filter.Wash the powder of gained with water one to twice, oven dry.Be put in the high temperature furnace and be heated to 700 ℃ under the nitrogen atmosphere, be incubated 3 hours.Promptly obtain the nickel oxide absorbent charcoal composite material, the content 45% of nickel oxide wherein, specific area 610m
2g
-1Under 25 ℃, 1g magnetic activated carbons composite can be removed the 295mg methylene blue at most.Adsorbent can use magnet to separate from solution fast.
Embodiment 7
Ultrasonic synthetic 38% MnO that contains
2Magnetic active carbon composite material.
The active carbon bubble was stirred 4 hours under 80 ℃ in the 63wt% red fuming nitric acid (RFNA), filter, washing.Take by weighing above active carbon 5g, be dissolved in 200ml, in the liquor potassic permanganate of 0.5M, stir.Under the room temperature ultrasonic 2 hours, filter.Wash the powder of gained with water one to twice, oven dry.Be put in the high temperature furnace and be heated to 550 ℃ under the nitrogen atmosphere, be incubated 1 hour.Promptly obtain the manganese oxide absorbent charcoal composite material, the content 38% of manganese oxide wherein, specific area 600m
2g
-1Through test, composite has magnetic.
Embodiment 8
The ultrasonic synthetic magnetic active carbon composite material that contains 23% MnFe2O4.
The active carbon bubble was stirred 3 hours under 90 ℃ in the 63wt% red fuming nitric acid (RFNA), filter, washing.Take by weighing above active carbon 5g, be dissolved in 200ml, the potassium permanganate of 0.5M and the mixed solution of iron chloride (mol ratio 1:2) stir.Under the room temperature ultrasonic 4 hours, filter.Wash the powder of gained with water one to twice, oven dry.Be put in the high temperature furnace and be heated to 600 ℃ under the nitrogen atmosphere, be incubated 4 hours.Promptly obtain the MnFe2O4 absorbent charcoal composite material, the content 23% of MnFe2O4 wherein, specific area 720m
2g
-1Through test, use magnet the absorbent charcoal composite material that is dispersed in the solution can be separated from solution.
Claims (7)
1, a kind of preparation method of magnetic active carbon composite material for water processing is characterized in that, comprises the steps:
The first step stirs the Powdered Activated Carbon material in nitric acid, wash with deionized water, and is dry then;
Second step took by weighing the absorbent charcoal material after the first step is handled, join in the metal salt solution, the mole dosage of slaine be absorbent charcoal material amount of substance 0.2-2.88 doubly, at room temperature ultrasonic, obtain powder sample, wash with water, dry then;
The 3rd step, the second step gained material is put into high temperature furnace, be heated to 500-800 ℃ under the blanket of nitrogen, insulation, obtain magnetic active carbon composite material at last, the percentage by weight of the magnetic material in this composite is 15-50%, and the percentage by weight of absorbent charcoal material is 85-50%.
2, the preparation method of magnetic active carbon composite material for water processing according to claim 1 is characterized in that, described stirring, and its temperature is 70-90 ℃, mixing time 1-6 hour.
3, the preparation method of magnetic active carbon composite material for water processing according to claim 1 and 2 is characterized in that, described stirring, and its time is 3-5 hour.
4, the preparation method of magnetic active carbon composite material for water processing according to claim 1, it is characterized in that, described metal salt solution, slaine wherein is for generating one or more the combination of slaine of magnetic metal or metal oxide by ultrasonic method.
According to the preparation method of claim 1 or 4 described magnetic active carbon composite material for water processing, it is characterized in that 5, described metal salt solution, slaine wherein are one or more the combination in iron, nickel or the manganese slaine.
6, the preparation method of magnetic active carbon composite material for water processing according to claim 1 is characterized in that, and is described at room temperature ultrasonic, 0.25-4 hour its time.
7, the preparation method of magnetic active carbon composite material for water processing according to claim 1 is characterized in that, described insulation, and its time is 1-5 hour.
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| CN116351392A (en) * | 2023-03-08 | 2023-06-30 | 农业农村部农业生态与资源保护总站 | Modified straw biochar and preparation method thereof and application of modified straw biochar in adsorption of heavy metals |
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